• 한국진공학회:학술대회논문집
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• 한국진공학회 2016년도 제50회 동계 정기학술대회 초록집
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• pp.129-129
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• 2016

Graphene, as a single layer of $sp^2$-bonded carbon atoms packed into a 2D honeycomb crystal lattice, has attracted much attention due to its outstanding properties. In order to synthesize high quality graphene, transition metals, such as nickel and copper, have been widely employed as catalysts, which needs transfer to desired substrates for various applications. However, the transfer steps are not only complicated but also inevitably induce defects, impurities, wrinkles, and cracks of graphene. Furthermore, the direct synthesis of graphene on dielectric surfaces has still been a premature field for practical applications. Therefore, cost effective and concise methods for transfer-free graphene are essentially required for commercialization. Here, we report a facile transfer-free graphene synthesis method through nickel and carbon co-deposited layer. In order to fabricate 100 nm thick NiC layer on the top of $SiO_2/Si$ substrates, DC reactive magnetron sputtering was performed at a gas pressure of 2 mTorr with various Ar : $CH_4$ gas flow ratio and the 200 W DC input power was applied to a Ni target at room temperature. Then, the sample was annealed under 200 sccm Ar flow and pressure of 1 Torr at $1000^{\circ}C$ for 4 min employing a rapid thermal annealing (RTA) equipment. During the RTA process, the carbon atoms diffused through the NiC layer and deposited on both sides of the NiC layer to form graphene upon cooling. The remained NiC layer was removed by using a 0.5 M $FeCl_3$ aqueous solution, and graphene was then directly obtained on $SiO_2/Si$ without any transfer process. In order to confirm the quality of resulted graphene layer, Raman spectroscopy was implemented. Raman mapping revealed that the resulted graphene was at high quality with low degree of $sp^3$-type structural defects. Additionally, sheet resistance and transmittance of the produced graphene were analyzed by a four-point probe method and UV-vis spectroscopy, respectively. This facile non-transfer process would consequently facilitate the future graphene research and industrial applications.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2012년도 제43회 하계 정기 학술대회 초록집
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• pp.346-347
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• 2012

최근 화석연료 대체 에너지원으로서 자동차용으로 연구 개발 및 응용되고 있는 고분자 전해질 연료전지(PEMFC: Proton exchange membrane fuel cells)에서 분리판(Bipolar Plate)은 스택 전체 무게의 80%, 스택 가격의 60% 정도로 가장 높은 비중을 차지한다. 분리판은 연료와 산화제를 공급해주는 통로 및 전지 운전 중에 생성된 물을 제거하는 통로 역할과 anode, cathode로서 전극 역할을 통해 스택 전력을 형성하는 핵심 기능과 전지와 전지 사이의 지지대 역할을 한다. 따라서 분리판은 전기전도성, 내부식성 및 기계적 특성이 우수해야함은 물론이고, 얇고 가벼우며 가공성이 뛰어나야 한다. 현재 가장 많이 사용되고 있는 금속 분리판 소재 중 스테인리스 스틸은 전기적, 기계적 특성 및 내부식성이 우수한 반면, 가격이 비싸고, 중량이 무거운 단점이 있다. 따라서 본 연구에서는 DC 반응성 마그네트론 스퍼터링법으로 전기적, 기계적 특성 및 내부 식성이 우수한 TiN, TiCN 박막을 스테인리스에 비해 중량이 1/3, 소재 단가가 1/4인 알루미늄 기판 위에 증착하여 박막 물성을 평가하였다. DC Power는 400 W, 기판과 타겟 사이의 거리는100 mm, 공정 압력은 0.5 Pa로 고정하였고, 3 inch의 지름과 순도 99.95%를 갖는 티타늄 타겟을 사용하였다. 공정 가스는 Ar을 주입하였으며, 질소와 탄소의 공급원으로는 질소($N_2$)와 메탄($CH_4$) 가스를 사용하여 챔버 내 주입혼합가스의 전체 유량을 50 sccm으로 고정시켰다. 증착된 박막의 전기적, 기계적 특성을 측정하였고, X-ray diffraction (XRD), Scanning electron microscope (SEM)을 이용하여 박막의 미세구조 및 표면 상태를 확인하였다. 또한, 내부식 특성을 평가하기 위해 potentiostatic, potentiodynamic 법을 이용하여 박막의 부식저항을 측정하였다. 증착된 TiN 박막의 경우 질소 함량의 증가에 따라 박막 증착속도는 감소하는 경향을 보였다. 이는 타겟 부근의 질소 라디칼 비율이 증가함에 따라 질화반응이 촉진된 것으로 생각된다. 또한, 증착된 TiN과 TiCN 박막은 반응성 질소 유량과 탄소 유량에 따라 각각 다른 미세구조를 가지는 것을 확인하였다. TiN과 TiCN은 NaCl형의 면심입방격자(FCC)로 같은 구조이며, 격자상수가 비슷하여 전율고용되어 TiCN을 형성하고, 탄소와 질소의 비에 따라 전기적 기계적 특성이 달라짐을 확인하였다.

• Bulletin of the Korean Chemical Society
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• 제35권7호
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• pp.2143-2147
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• 2014

Ketene-forming elimination from 2-X-4-nitrophenyl furylacetates (1a-d) promoted by $R_2NH-R_2NH_2{^+}$ in 70 mol % MeCN(aq) has been studied kinetically. When X = Cl and $NO_2$, the reactions exhibited second-order kinetics as well as Br$\ddot{o}$nsted ${\beta}$ = 0.37-0.54 and $|{\beta}_{lg}|$ = 0.31-0.45. The Br$\ddot{o}$nsted ${\beta}$ decreased with a poorer leaving group and $|{\beta}_{lg}|$ increased with a weaker base. The results are consistent with an E2 mechanism. When the leaving group was changed to a poorer one [X= H (1a) and $OCH_3$ (1b)], the reaction mechanism changed to the competing E2 and E1cb mechanisms. A further change to the E1cb mechanism was realized for the reaction of 1a with $i-Pr_2NH/i-Pr_2NH_2{^+}$ in 70 mol % MeCN-30 mol % $D_2O$. By comparing the kinetic results in this study with the existing data for $ArCH_2C(O)OC_6H_3-2-X-4-NO_2$, the effect of the ${\beta}$-aryl group on the ketene-forming elimination was assessed.

• 한국광학회:학술대회논문집
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• 한국광학회 2005년도 하계학술발표회
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• pp.28-29
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• 2005

본 논문에서는 MEH-PPV와 DFPP의 폴리머 물질을 이용하여 photovoltaic device가 제작되었고, 그림 1에 두 물질의 분자 구조가 보여진다. Photovoltaic cell의 전기-광학적 특성은 활성층의 폴리머 물질에 의해 결정된다. 이러한 특성을 알아보기 위해서 홉수 스펙트럼이 측정되었다. DFPP는 chloroform, chlorobenzen, THF, acetone에 잘 녹았으며, 본 논문에서는 chloroform이 용매로 사용되었다. 제작 공정은 다음과 같다. 인듐 주석 산화물 (ITO)이 증착된 유리기판은 photolithography 공정을 거친 후, 왕수(HNO$_{3}$ + HCL)로 식각됨으로서 전극의 패턴이 제작되었다. 그리고 ITO 전극 패턴 된 유리기판 위에 PEDOT (CH8000, Baytron)이 코팅된 후 Ar이 주입되는 Convection Oven을 이용하여 120$^{\circ}$C에서 2시간 동안 열처리되어 수분이 제거되었다. 활성층에는 MEH-PPV와 DFPP가 9:1과 2.33:1로 혼합된 폴리머가 사용되었고, 이것은 0.3 %w.t.가 되도록 chloroform에 넣어 5시간 동안 스핀바를 돌려서 용해되었다. 이 용액은 ITO 전극 패턴이 형성된 글라스 위에 3000 rpm으로 45 초간 스핀코팅 되었다. 이 때 얻어진 유기물 박막층은 80$^{\circ}$C의 Ar이 주입되는 convection oven에서 3시간 동안 경화되었다. 경화된 단층 유기물 박막층 위에 Li-Al이 1000 ${\AA}$의 두께로 증착되어 전극이 형성되었고, 이후 질소가 채워진 globe box에서 소자는 encapsulation되어 산소와 수분에 대한 영향으로부터 차단되었다. 상기의 공정으로 제작된 소자의 박막구조는 그림 2에서 보여진다. 그림 3은 MEH-PPV와 DFPP를 혼합했을 때의 흡수 스펙트럼이다. 최대 흡수 파장은 511 nm였다. 그리고 photovoltaic cell의 V-I 특성 결과가 그림 4와 같이 측정되었다. 측정에서는 300${\sim}$700 nm의 파장대를 갖는 태양광 모사계가 사용되었고, 셀의 면적은 10 mm$^{2}$였다. 그림 5의 I-V 특성으로부터 MEH-PPV와 DFPP가 9:1 로 혼합했을 때보다 2.33:1 로 혼합했을 때, photovoltaic device의 효율이 향상됨을 확인할 수 있다. 빛이 75 mW/cm$^{2}$ 의 세기로 조사될 때 9:1과 2.33:1로 혼합된 소자의 open circuit voltage (V$_{oc}$)는 비슷하지만, short circuit current Density (J$_{sc}$)는 각각 -1.39 ${\mu}$A/cm$^{2}$ 와 -3.72${\mu}$A/cm$^{2}$ 로 약 2.7배 정도 증가되었음을 볼 수 있다. 이러한 결과를 통해 electron acceptor인 DFPP의 비율이 높아질수록 photovoltaic cell의 conversion efficiency가 더 크게 됨을 확인할 수 있다. 그러므로 효율이 최대가 되는 두 폴리머의 혼합 비율이 최적화되는 조건을 찾는 것은 매우 중요한 연구가 될 것이다.

• 한국재료학회지
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• 제9권11호
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• pp.1129-1136
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• 1999

TEMAT precursor를 사용하여 다양한 증착 조건으로 ICP-CVD 방법으로 Si(100) 기판 위에 TiN 박막을 형성하였다. 형성된 TiN 박막의 결정상, 미세구조, 그리고 전기적 특성은 XRD, XPS, HRTEM, 그리고 전기적 측정으로 특성을 조사하였다. BI 구조를 갖는 다결정 TiN 박막은 기판의 온도가 $200^{\circ}C$ 이상의 온도에서 형성되었다. TiN(111) 박막은 기판의 온도가 $300^{\circ}C$에서 TEMAT, $\textrm{N}_{2}$, 그리고 Ar 가스의 유량이 10, 5, 그리고 5sccm으로 반응로에 주입할 때 형성되었다. TiN/Si(100) 계면은 TiN과 $\textrm{SiO}_2$사이에 계면반응이 없었으며 평탄하였다. 기판의 온도가 $500^{\circ}C$에서 형성된 TiN 박막의 비저항, carrier 농도와 이동도는 21 $\mu\Omega$cm, 9.5$\times\textrm{10}^{18}\textrm{cm}^{-3}$와 $462.6\textrm{cm}^{2}$/Vs으로 주어졌다.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2015년도 제49회 하계 정기학술대회 초록집
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• pp.109.2-109.2
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• 2015

Graphene, as a single layer of $sp^2$-bonded carbon atoms packed into a 2D honeycomb crystal lattice, has attracted much attention due to its outstanding properties such as high carrier mobility, chemical stability, and optical transparency. In order to synthesize high quality graphene, transition metals, such as nickel and copper, have been widely employed as catalysts, which need transfer to desired substrates for various applications. However, the transfer steps inevitably induce defects, impurities, wrinkles, and cracks of graphene. Here, we report a facile transfer-free graphene synthesis method through nickel and carbon co-deposited layer, which does not require separately deposited catalytic nickel and carbon source layers. The 100 nm NiC layer was deposited on the top of $SiO_2/Si$ substrates by nickel and carbon co-deposition. When the sample was annealed at $1000^{\circ}C$, the carbon atoms diffused through the NiC layer and deposited on both sides of the layer to form graphene upon cooling. The remained NiC layer was removed by using nickel etchant, and graphene was then directly obtained on $SiO_2/Si$ without any transfer process. Raman spectroscopy was carried out to confirm the quality of resulted graphene layer. Raman spectra revealed that the resulted graphene was at high quality with low degree of $sp^3$-type structural defects. Furthermore, the Raman analysis results also demonstrated that gas flow ratio (Ar : $CH_4$) during the NiC deposition and annealing temperature significantly influence not only the number of graphene layers but also structural defects. This facile non-transfer process would consequently facilitate the future graphene research and industrial applications.

• 한국재료학회지
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• 제24권12호
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• pp.694-699
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• 2014

We report the chemical vapor deposition growth characteristics of graphene on various catalytic metal substrates such as Ni, Fe, Ag, Au, and Pt. 50-nm-thick metal films were deposited on $SiO_2/Si$ substrates using dc magnetron sputtering. Graphene was synthesized on the metal/$SiO_2$/Si substrates with $CH_4$ gas (1 SCCM) diluted in mixed gases of 10% $H_2$ and 90 % Ar (99 SCCM) using inductively-coupled plasma chemical vapor deposition (ICP-CVD). The highest quality of graphene film was achieved on Ni and Fe substrates at $900^{\circ}C$ and 500 W of ICP power. Ni substrate seemed to be the best catalytic material among the tested materials for graphene growth because it required the lowest growth temperature ($600^{\circ}C$) as well as showing a low ICP power of 200W. Graphene films were successfully grown on Ag, Au, and Pt substrates as well. Graphene was formed on Pt substrate within 2 sec, while graphene film was achieved on Ni substrate over a period of 5 min of growth. These results can be understood as showing the direct CVD growth of graphene with a highly efficient catalytic reaction on the Pt surface.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2008년도 추계학술대회 논문집 Vol.21
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• pp.51-51
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• 2008

Carbon nanotubes (CNTs) have long been reported as an ideal material due to their excellent electrical conductivity and chemical and mechanical stability as well as their high aspect ratios for field emission devices. CNT emitters made by screen printing the organic binder-based CNT paste may act as a source to release gases inside a vacuum panel. These residual gases may cause a catastrophic damage by electrical arcing or ion bombardment to the vacuum microelectronic devices and may change their physical or electrical properties by adsorbing on the CNT emitter surface. In this study, we analyzed the composition of residual gases inside the vacuum-sealed panel by residual gas analyzer (RGA), investigating the effects of individual gases of different kinds at several pressures on the field emission characteristics of CNT emitters. The residual gases included $H_2$, CO, $CO_2$, $N_2$, $CH_4$, $H_2O$, $C_2H_6$, and Ar. Effect of residual gases on the field emission was studied by observing the variation of the pulse voltages with the duty ratio of3.3% to keep the constant emission current of $28{\mu}A$. Each gas species was introduced to a vacuum chamber up to three different pressures ($5\times10^{-7}$, $5\times10^{-6}$, and $5\times10^{-5}$ torr) each for 1 h while electron emission was continued. The three different pressure regions were separated by keeping a high vacuum of $\sim10^{-8}$ torr for a 1 h. The emission was terminated 6 h after the third gas exposure was completed. Field emission characteristics under residual gases will be discussed in terms of their adsorption and desorption on the surface of CNTs and the resultant change of work function.

• 한국재료학회지
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• 제23권1호
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• pp.47-52
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• 2013

Graphene has been synthesized on 100- and 300-nm-thick Ni/$SiO_2$/Si substrates with $CH_4$ gas (1 SCCM) diluted in mixed gases of 10% $H_2$ and 90% Ar (99 SCCM) at $900^{\circ}C$ by using inductively-coupled plasma chemical vapor deposition (ICP-CVD). The film morphology of 100-nm-thick Ni changed to islands on $SiO_2$/Si substrate after heat treatment at $900^{\circ}C$ for 2 min because of grain growth, whereas 300-nm-thick Ni still maintained a film morphology. Interestingly, suspended graphene was formed among Ni islands on 100-nm-thick Ni/$SiO_2$/Si substrate for the very short growth of 1 sec. In addition, the size of the graphene domains was much larger than that of Ni grains of 300-nm-thick Ni/$SiO_2$/Si substrate. These results suggest that graphene growth is strongly governed by the direct formation of graphene on the Ni surface due to reactive carbon radicals highly activated by ICP, rather than to well-known carbon precipitation from carbon-containing Ni. The D peak intensity of the Raman spectrum of graphene on 300-nm-thick Ni/$SiO_2$/Si was negligible, suggesting that high-quality graphene was formed. The 2D to G peak intensity ratio and the full-width at half maximum of the 2D peak were approximately 2.6 and $47cm^{-1}$, respectively. The several-layer graphene showed a low sheet resistance value of $718{\Omega}/sq$ and a high light transmittance of 87% at 550 nm.

• 한국표면공학회지
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• 제48권6호
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• pp.297-302
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• 2015

Nanocrystalline diamond(NCD) coated aluminium plates were prepared and applied as heat sinks for LED modules. NCD films were deposited on 1 mm thick Al plates for times of 2 - 10 h in a microwave plasma chemical vapor deposition reactor. Deposition parameters were the microwave power of 1.2 kW, the working pressure of 90 Torr, the $CH_4/Ar$ gas ratio of 2/200 sccm. In order to enhance diamond nucleation, DC bias voltage of -90 V was applied to the substrate during deposition without external heating. NCD film was identified by X-ray diffraction and Raman spectroscopy. The Al plates with about 300 nm thick NCD film were attached to LED modules and thermal analysis was carried out using Thermal Transient Tester (T3ster) in a still air box. Thermal resistance of the module with NCD/Al plate was 3.88 K/W while that with Al plate was 5.55 K/W. The smaller the thermal resistance, the better the heat emission. From structure function analysis, the differences between junction and ambient temperatures were $12.1^{\circ}C$ for NCD/Al plate and $15.5^{\circ}C$ for Al plate. The hot spot size of infrared images was larger on NCD/Al than Al plate for a given period of LED operation. In conclusion, NCD coated Al plate exhibited better thermal spreading performance than conventional Al heat sink.